EP0027917A1 - Réactif et procédé pour la détermination d'hydrazine - Google Patents
Réactif et procédé pour la détermination d'hydrazine Download PDFInfo
- Publication number
- EP0027917A1 EP0027917A1 EP80105954A EP80105954A EP0027917A1 EP 0027917 A1 EP0027917 A1 EP 0027917A1 EP 80105954 A EP80105954 A EP 80105954A EP 80105954 A EP80105954 A EP 80105954A EP 0027917 A1 EP0027917 A1 EP 0027917A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- hydrazine
- dimethylaminocinnamaldehyde
- solution
- determination
- reagent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 title abstract description 7
- RUKJCCIJLIMGEP-ONEGZZNKSA-N 4-dimethylaminocinnamaldehyde Chemical compound CN(C)C1=CC=C(\C=C\C=O)C=C1 RUKJCCIJLIMGEP-ONEGZZNKSA-N 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- -1 ethylene glycol monoalkyl ether Chemical class 0.000 claims description 5
- 239000012488 sample solution Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 14
- BGNGWHSBYQYVRX-UHFFFAOYSA-N 4-(dimethylamino)benzaldehyde Chemical compound CN(C)C1=CC=C(C=O)C=C1 BGNGWHSBYQYVRX-UHFFFAOYSA-N 0.000 description 7
- 239000011521 glass Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000036651 mood Effects 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003142 primary aromatic amines Chemical class 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 150000003336 secondary aromatic amines Chemical class 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1826—Organic contamination in water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/17—Nitrogen containing
- Y10T436/173845—Amine and quaternary ammonium
Definitions
- the invention relates to a stable reagent and a method for the determination of hydrazine in aqueous solutions.
- Hydrazine is a well-known anti-corrosion agent for steel in contact with water, e.g. B. in steam boiler operation, in hot water circulation systems, the preservation of containers at standstill etc.
- 0.1-300 ppm of hydrazine are added to the water, systems with higher pressures and temperatures requiring the lowest amounts of hydrazine.
- the residual hydrazine content in the range below 0.1 ppm represents an important parameter in boiler operation, since this determines the time and the extent of the hydrazine replenishment.
- 4-dimethylaminobenzaldehyde unlike 4-dimethylaminobenzaldehyde, 4-dimethylaminocinnamaldehyde has poor durability in solution. A good shelf life is absolutely necessary for a liquid ready-to-use reagent so that it is not necessary to prepare a freshly prepared reagent solution before each determination.
- the invention was therefore based on the object of a stable, sensitive reagent and a method for loading to provide the mood of hydrazine in aqueous solutions with which the lowest hydrazine contents can still be reliably detected.
- the invention relates to an agent for the determination of hydrazine in aqueous solutions, which contains 4-dimethylaminocinnamaldehyde.
- the agent is preferably in the form of a 2 to 4% strength, in particular a 3% strength solution of 4-dimethylaminocinnamaldehyde in ethylene glycol monoalkyl ether, in particular ethylene glycol monoethyl ether.
- Another object of the invention is a method for determining hydrazine in aqueous solutions, which is characterized in that a solution of 4-dimethylaminocinnamaldehyde in ethylene glycol monoalkyl ether is added to the hydrazine-containing sample solution and the content of 4-dimethylaminocinnamaldehyde-azine formed is determined colorimetrically.
- the increase in the reaction contrast with the aid of the agent according to the invention leads to color series from yellow to orange to wine red, which enable a ten-fold gradation and can be measured optically equally well in daylight as well as in artificial light.
- the high reaction contrast ( ⁇ ) of 135 nm is also advantageous for the photometric measurement compared to the conventional method with 4-dimethylaminobenzaldehyde of only 45 nm. Since the extinction maximum of 540 nm is in the red range and due to a yellowish natural water color hardly affected - the color compensation samples necessary in these cases, in which the hydrazine has to be eliminated in an additional batch, become superfluous.
- Hydrazine is determined by acidifying the sample solution and adding the solution of 4-dimethylaminocinnamaldehyde in ethylene glycol monoalkyl ether. All acids which do not interfere with the determination can be used for acidification, preferably mineral acids such as sulfuric acid, hydrochloric acid, perchloric acid, phosphoric acid etc. Mixtures of sulfuric acid and perchloric acid have proven particularly suitable.
- the visual or spectrophotometric test takes place after 5 to 20 minutes. Evaluation. If the determination is made in a round-bottom glass, the visual evaluation is carried out using a color scale; 0.01 ppm of hydrazine can still be reliably detected. If the determination is carried out in a cuvette, the spectrophotometric measurement is carried out at 540 nm.
- a solution which can contain between 0.2 and 4 ppm hydrazine, 0.2 ml of a sulfuric acid / perchloric acid mixture (7 parts of 25% sulfuric acid and 3 parts of 70% Perchloric acid) and 0.15 ml of a 3% solution of 4-dimethylaminocinnamaldehyde in ethylene glycol monoethyl ether.
- the glass After thorough mixing and a standing time of about 10 minutes, the glass is fixed over a white surface; Seen from above, a clear color gradation from yellow to red can be seen, which can be clearly assigned to the hydrazine contents using a color scale.
- a solution which can contain between 0.02 and 0.25 ppm hydrazine, 0.4 ml of a sulfuric acid / perchloric acid mixture (7 parts of 25% sulfuric acid and 3 parts of 70% perchloric acid) and 0.3 ml of a 3% solution of 4-dimethylamino cinnamaldehyde in ethylene glycol monoethyl ether.
- a sulfuric acid / perchloric acid mixture 7 parts of 25% sulfuric acid and 3 parts of 70% perchloric acid
- 0.3 ml of a 3% solution of 4-dimethylamino cinnamaldehyde in ethylene glycol monoethyl ether When viewed from above in flat-bottomed glass with a diameter of 20 mm on a white base, this results in a clear color gradation from yellow to orange-red. 'The hydrazine content can be determined precisely using a color scale.
- 0.2 ml of a sulfuric acid / perchloric acid mixture and 0.15 ml of a 3% solution of 4-dimethylaminocinnamaldehyde in ethylene glycol monoethyl ether are added to 5 ml of a solution, which may contain between 0.05 and 4.5 ppm hydrazine.
- a solution which may contain between 0.05 and 4.5 ppm hydrazine.
- the staining is measured in a cuvette with a layer thickness of 10 mm at 540 nm in a spectrophotometer against a blank sample prepared at the same time.
- the concentration of hydrazine is read on the basis of the measured absorbance value from a calibration curve previously known with hydrazine solutions.
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Biophysics (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2942960 | 1979-10-24 | ||
| DE19792942960 DE2942960A1 (de) | 1979-10-24 | 1979-10-24 | Reagenz und verfahren zur bestimmung von hydrazin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0027917A1 true EP0027917A1 (fr) | 1981-05-06 |
| EP0027917B1 EP0027917B1 (fr) | 1984-10-10 |
Family
ID=6084267
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP80105954A Expired EP0027917B1 (fr) | 1979-10-24 | 1980-10-02 | Réactif et procédé pour la détermination d'hydrazine |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US4395494A (fr) |
| EP (1) | EP0027917B1 (fr) |
| DE (2) | DE2942960A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114636695A (zh) * | 2022-05-18 | 2022-06-17 | 广东江门中医药职业学院 | 一种预包装制品使用不合格鱼肉原料的检测方法 |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4775633A (en) * | 1984-04-26 | 1988-10-04 | Thermedics Inc. | Detection of hydrazine compounds in gaseous samples by their conversion to nitric oxide-yielding derivatives |
| US20060084176A1 (en) * | 2004-04-01 | 2006-04-20 | Yissum Research Development Company Of The Hebrew University Of Jerusalem | Detection of uronium salts |
| CN103018241B (zh) * | 2012-12-17 | 2015-06-10 | 兰州大学 | 一种半定量快速检测水中肼含量的方法 |
| RU2613304C2 (ru) * | 2015-01-26 | 2017-03-15 | Федеральное государственное казенное военное образовательное учреждение высшего профессионального образования "Военная академия материально-технического обеспечения имени генерала армии А.В. Хрулёва" Министерства обороны Российской Федерации | Способ определения наличия гидразинных и аминных горючих ракетных топлив |
| US11713877B2 (en) * | 2018-05-04 | 2023-08-01 | Donaldson Company, Inc. | Systems and methods for removing organic compounds from steam |
| US11649178B2 (en) | 2019-10-15 | 2023-05-16 | Donaldson Company, Inc. | Systems and methods for removing organic compounds from water used to generate steam |
| WO2021226305A1 (fr) * | 2020-05-06 | 2021-11-11 | Syngenta Crop Protection Ag | Mesure colorimétrique du fludioxonil |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3424845A (en) * | 1967-05-25 | 1969-01-28 | Salsbury Lab | 3,5-dinitrosalicylic acid, 5-nitrofurfurylidene hydrazide and compositions containing and methods employing the same for the control of histomoniasis |
| US3549329A (en) * | 1967-08-23 | 1970-12-22 | Trw Inc | Sensors for detecting reducing vapors |
| US3621095A (en) * | 1968-06-21 | 1971-11-16 | Salsbury Lab | Composition for treating histomoniasis in poultry |
| US4200608A (en) * | 1978-06-15 | 1980-04-29 | The United States Of America As Represented By The Secretary Of The Army | Detector for fumes of hydrazine and its derivatives |
-
1979
- 1979-10-24 DE DE19792942960 patent/DE2942960A1/de not_active Withdrawn
-
1980
- 1980-10-02 EP EP80105954A patent/EP0027917B1/fr not_active Expired
- 1980-10-02 DE DE8080105954T patent/DE3069422D1/de not_active Expired
- 1980-10-24 US US06/200,249 patent/US4395494A/en not_active Expired - Lifetime
Non-Patent Citations (2)
| Title |
|---|
| CHEMICAL ABSTRACTS, Band 83, 1975, Columbus, Ohio, USA, E.J. DIXON et al. "Determination of unsulfonated primary aromatic amines in water-soluble food dyes and other food additives" Seite 380, Zusammenfassung Nr. 130 105n * |
| CHEMICAL ABSTRACTS, Band 83, 1975, Columbus, Ohio, USA, M. MATSUTANI: "Measuring content of urea nitrogenin serum" Seite 270, Zusammenfassung Nr. 175 162v * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114636695A (zh) * | 2022-05-18 | 2022-06-17 | 广东江门中医药职业学院 | 一种预包装制品使用不合格鱼肉原料的检测方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0027917B1 (fr) | 1984-10-10 |
| DE3069422D1 (en) | 1984-11-15 |
| US4395494A (en) | 1983-07-26 |
| DE2942960A1 (de) | 1981-05-07 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
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| AK | Designated contracting states |
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| 17P | Request for examination filed |
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| GRAA | (expected) grant |
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| REF | Corresponds to: |
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| ET | Fr: translation filed | ||
| PLBE | No opposition filed within time limit |
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| STAA | Information on the status of an ep patent application or granted ep patent |
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| 26N | No opposition filed | ||
| PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
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| GBPC | Gb: european patent ceased through non-payment of renewal fee | ||
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